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Pyridine → 2-[2-(tert-Butyl-dimethyl-silanyloxy)-ethyl]-(5-tert-butyl-2H-pyrazol-3-yl)-carbamic acid 2,2,2-trichloro-ethyl ester

HRID 1446654
ノート
印刷プレビュー

反応式

HRID 1446654 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([NH2:20])[N:8]([CH2:10][CH2:11][O:12][Si:13]([C:16]([CH3:19])([CH3:18])[CH3:17])([CH3:15])[CH3:14])[N:9]=1)([CH3:4])([CH3:3])[CH3:2].N1C=CC=CC=1.Cl[C:28]([O:30][CH2:31][C:32]([Cl:35])([Cl:34])[Cl:33])=[O:29].C(OCC)(=O)C>C1COCC1.O>[Cl:33][C:32]([Cl:35])([Cl:34])[CH2:31][O:30][C:28](=[O:29])[NH:20][C:7]1[N:8]([CH2:10][CH2:11][O:12][Si:13]([C:16]([CH3:19])([CH3:18])[CH3:17])([CH3:14])[CH3:15])[N:9]=[C:5]([C:1]([CH3:4])([CH3:2])[CH3:3])[CH:6]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 1049PyridineHCID 8857Ethyl AcetateHCID 870632,2,2-Trichloroethyl chloroformateHCID 685465445-tert-Butyl-2-[2-(tert-butyl-dimethyl-silanyloxy)-ethyl]-2H-pyrazol-3-ylamine

生成物 1

HCID 685422102-[2-(tert-Butyl-dimethyl-silanyloxy)-ethyl]-(5-tert-butyl-2H-pyrazol-3-yl)-carbamic acid 2,2,2-trichloro-ethyl ester収率 100%

試薬・触媒・溶媒

2
HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

Dissolve 5-tert-butyl-2-[2-(tert-butyl-dimethyl-silanyloxy)-ethyl]-2H-pyrazol-3-ylamine (5.5 g, 0.018 mol) in THF (100 mL) under N2 and cool to 0° C. Add pyridine (1.6 mL, 1.1 equiv.) via syringe followed by dropwise addition of 2,2,2-trichloroethyl chloroformate (2.7 mL, 1.1 equiv.). Stir the reaction at 0° C. for one hour then remove the cooling bath and allow the reaction to stir for a total of 5 hours. Dilute the reaction with ethyl acetate and water. Wash the organic layer with water then saturated aqueous saturated sodium chloride and then dry over magnesium sulfate, filter, and concentrate in vacuo to give a residue (8.7 g, 100%) that is used without further purification. MS (ES), m/z 474 (M+1).

後処理

  1. customthe reaction at 0° C. for one hour
  2. customthen remove the cooling bath
  3. customthe reaction
  4. stirringto stir for a total of 5 hours
  5. additionDilute
  6. washWash the organic layer with water
  7. dry with materialsaturated aqueous saturated sodium chloride and then dry over magnesium sulfate
  8. filtrationfilter
  9. concentrationconcentrate in vacuo

出典と根拠

ORDレコード
ord-1cc696cb95e44dee9e7e38a7c65012dd
出典データセット
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07666879B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート